Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl trifluoroacetate | HCID 9794 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 67982928 | HCID 67982928 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67983207 | HCID 67983207 | — |
Reaction Steps
1.41 g (35.3 mmol) of sodium hydride are initially charged in absolute THF (50 ml), and 4.05 g (17.6 mmol) of [3,5-dichloro-4-(dimethylamino)phenyl]acetonitrile in 20 ml of absolute THF are added dropwise at 0° C. The mixture is stirred at 0° C. for 20 minutes, and 5.02 g (35.3 mmol) of ethyl trifluoroacetate are then added dropwise at 0° C. The reaction mixture is warmed to room temperature and then carefully added to water. After washing with n-hexane, the aqueous phase is acidified with 1 N HCl. A colourless solid precipitates out and is, after filtration with suction and air-drying, used without further purification for the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09066945B2 |
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| Source dataset | uspto-grants-2015_06 |
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| ORD ID | ord-aa9139cae5ac4c1787cef21cf49b5990 |
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| Source note | uspto-grants-2015_06 |
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